P
US9305715B2ActiveUtilityPatentIndex 92

Method of formulating perovskite solar cell materials

Assignee: HUNT ENERGY ENTPR LLCPriority: Aug 1, 2014Filed: May 13, 2015Granted: Apr 5, 2016
Est. expiryAug 1, 2034(~8.1 yrs left)· nominal 20-yr term from priority
Inventors:IRWIN MICHAEL DCHUTE JERRED ADHAS VIVEK V
H01G 9/2045Y02E10/549B05D 3/107B05D 1/38Y02E10/542H01G 9/2009H10K 85/50H10K 30/451H10K 71/12H10F 77/124H01L 31/032H10K 30/15H03K 17/223H03K 5/2472H03K 5/19H10K 71/40H10F 71/128H10F 77/311H10F 77/12H10K 85/30H10K 30/151Y02E10/544
92
PatentIndex Score
21
Cited by
11
References
30
Claims

Abstract

A method for preparing photoactive perovskite materials. The method comprises the step of preparing a lead halide precursor ink. Preparing a lead halide precursor ink comprises the steps of: introducing a lead halide into a vessel, introducing a first solvent to the vessel, and contacting the lead halide with the first solvent to dissolve the lead halide. The method further comprises depositing the lead halide precursor ink onto a substrate, drying the lead halide precursor ink to form a thin film, annealing the thin film, and rinsing the thin film with a second solvent and a salt.

Claims

exact text as granted — not AI-modified
What is claimed is: 
     
       1. A method comprising the steps of:
 preparing a lead halide precursor ink, wherein preparing a lead halide precursor ink comprises the steps of:
 introducing a lead halide into a vessel, wherein the lead halide comprises a mixture of lead (II) chloride and lead (II) iodide; 
 introducing a first solvent to the vessel; and 
 contacting the lead halide with the first solvent to dissolve the lead halide to form the lead halide precursor solution; 
 
 depositing the lead halide precursor ink onto a substrate; 
 drying the lead halide precursor ink to form a thin film; 
 annealing the thin film; and 
 rinsing the thin film with a second solvent and a salt selected from the group consisting of methylammonium iodide, formamidinium iodide, guanidinium iodide, 1,2,2-triaminovinylammonium iodide, and 5-aminovaleric acid hydroiodide. 
 
     
     
       2. The method of  claim 1 , wherein the mixture of lead (II) chloride and lead (II) iodide is mixed in a ratio of 10 mol of lead (II) chloride to 90 mol of lead (II) iodide. 
     
     
       3. The method of  claim 1 , wherein the first solvent is selected from the group consisting of dry dimethylformamide, dimethylsulfoxide (DMSO), methanol, ethanol, propanol, butanol, tetrahydrofuran, formamide, pyridine, pyrrolidine, chlorobenzene, dichlorobenzene, dichloromethane, chloroform, and combinations thereof. 
     
     
       4. The method of  claim 1 , wherein contacting the lead halide with the solvent to dissolve the lead halide occurs between about 20° C. to about 150° C. 
     
     
       5. The method of  claim 1 , wherein contacting the lead halide with the solvent to dissolve the lead halide occurs at about 85° C. 
     
     
       6. The method of  claim 1 , wherein the lead halide precursor ink has a concentration of the lead halide between about 0.001M and about 10M. 
     
     
       7. The method of  claim 1 , wherein depositing the lead halide precursor ink onto the substrate occurs by drop casting, spin casting, slot-die printing, screen printing, or ink-jet printing. 
     
     
       8. The method of  claim 1 , wherein annealing the thin film occurs for up to 24 hours at a temperature between about 20° C. to about 300° C. 
     
     
       9. The method of  claim 1 , wherein annealing the thin film occurs for about ten minutes at a temperature of about 50° C. 
     
     
       10. The method of  claim 1 , wherein the second solvent selected from the group consisting of dimethylformamide, isopropanol, methanol, ethanol, butanol, chloroform, chlorobenzene, dimethylsulfoxide, water, and combinations thereof. 
     
     
       11. The method of  claim 1 , wherein the salt comprises formamidinium iodide. 
     
     
       12. The method of  claim 10 , wherein the salt is dissolved in the second solvent in a concentration of between about 0.001 M and about 10M. 
     
     
       13. The method of  claim 1 , wherein the salt comprises methylammonium iodide. 
     
     
       14. The method of  claim 1 , wherein rinsing the thin film comprises at least partial submersion in the second solvent. 
     
     
       15. The method of  claim 1 , wherein annealing the thin film occurs for between about 5 to about 30 minutes at a temperature between about 40° C. to about 60° C. 
     
     
       16. A perovskite material prepared by a process comprising the steps of:
 preparing a lead halide precursor ink, wherein preparing a lead halide precursor ink comprises the steps of:
 introducing a lead halide into a vessel, wherein the lead halide comprises a mixture of lead (II) chloride and lead (II) iodide; 
 introducing a first solvent to the vessel; and 
 contacting the lead halide with the first solvent to dissolve the lead halide; 
 depositing the lead halide precursor ink onto a substrate; 
 drying the lead halide precursor ink to form a thin film; 
 annealing the thin film; and 
 
 rinsing the thin film with a second solvent and a salt selected from the group consisting of methylammonium iodide, formamidinium iodide, guanidinium iodide, 1,2,2-triaminovinylammonium iodide, and 5-aminovaleric acid hydroiodide to form the perovskite material. 
 
     
     
       17. The perovskite material of  claim 16 , wherein the mixture of lead (II) chloride and lead (II) iodide is mixed in a ratio of 10 mol of lead (II) chloride to 90 mol of lead (II) iodide. 
     
     
       18. The perovskite material of  claim 16 , wherein the first solvent is selected from the group consisting of dry dimethylformamide, dimethylsulfoxide (DMSO), methanol, ethanol, propanol, butanol, tetrahydrofuran, formamide, pyridine, pyrrolidine, chlorobenzene, dichlorobenzene, dichloromethane, chloroform, and combinations thereof. 
     
     
       19. The perovskite material of  claim 16 , wherein contacting the lead halide with the solvent to dissolve the lead halide occurs between about 20° C. to about 150° C. 
     
     
       20. The perovskite material of  claim 16 , wherein contacting the lead halide with the solvent to dissolve the lead halide occurs at about 85° C. 
     
     
       21. The perovskite material of  claim 16 , wherein the lead halide precursor ink has a concentration of the lead halide between about 0.001M and about 10M. 
     
     
       22. The perovskite material of  claim 16 , wherein depositing the lead halide precursor ink onto the substrate occurs by drop casting, spin casting, slot-die printing, screen printing, or ink-jet printing. 
     
     
       23. The perovskite material of  claim 16 , wherein annealing the thin film occurs for up to 24 hours at a temperature between about 20° C. to about 300° C. 
     
     
       24. The perovskite material of  claim 16 , wherein annealing the thin film occurs for about ten minutes at a temperature of about 50° C. 
     
     
       25. The perovskite material of  claim 16 , wherein the second solvent selected from the group consisting of dimethylformamide, isopropanol, methanol, ethanol, butanol, chloroform chlorobenzene, dimethylsulfoxide, water, and combinations thereof. 
     
     
       26. The perovskite material of  claim 16 , wherein the salt comprises formamidinium iodide. 
     
     
       27. The perovskite material of  claim 26 , wherein the salt is dissolved in the second solvent in a concentration of between about 0.001M and about 10M. 
     
     
       28. The perovskite material of  claim 16 , wherein the salt comprises methylammonium iodide. 
     
     
       29. The perovskite material of  claim 16 , wherein rinsing the thin film comprises at least partial submersion in the second solvent. 
     
     
       30. The perovskite material of  claim 16 , wherein annealing the thin film occurs for between about 5 to about 30 minutes at a temperature between about 40° C. to about 60° C.

Cited by (0)

No later patents cite this yet.

References (0)

No backward citations on record.